CN107469150A - A kind of implantation material for forming built-in electric field and preparation method thereof - Google Patents
A kind of implantation material for forming built-in electric field and preparation method thereof Download PDFInfo
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- CN107469150A CN107469150A CN201710666015.5A CN201710666015A CN107469150A CN 107469150 A CN107469150 A CN 107469150A CN 201710666015 A CN201710666015 A CN 201710666015A CN 107469150 A CN107469150 A CN 107469150A
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- Prior art keywords
- electric field
- implantation material
- strontium
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- ruthenic acid
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/10—Ceramics or glasses
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
Abstract
The present invention relates to a kind of implantation material for forming built-in electric field and preparation method thereof, the technical problem that current material does not possess enough bone-inducting actives and bone contact ratio is not high is which solved, it is made up of sandwich construction piezoceramic material.Invention also provides its preparation method.It the method can be widely used in bone-repairing composite material preparation field.
Description
Technical field
The present invention relates to a kind of surgical operation repair materials and preparation method thereof, more particularly to one kind can form in-built electrical
Implantation material of field and preparation method thereof.
Background technology
It is the Main Means for treating absence of tooth that plantation, which is repaired,.With social development and the raising of quality of life, planting body
Demand increase year by year.However, presently used planting body is because mechanical matching is poor, lacks the reasons such as bioactivity, shadow
Ring clinical long-time stability, Percentage bound, plantation reparation success rate.In recent years, although numerous studies are carried out to planting body material
Surface is modified, such as drug loading, surface micro-nano structure, but because drug half-life is short, micro-nano physical arrangement osteoinductive
Can deficiency and cause that bioactivity is poor, Integrated implant effect is undesirable, it is difficult to meet clinical repair demand.Therefore, how plantation is made
Body material surface possesses enough bone-inducting actives and improves bone contact ratio, turns into the main bottle of current oral implant rehabilitation material
Neck.
The content of the invention
The present invention is exactly to solve the technology that current material does not possess enough bone-inducting actives and bone contact ratio is not high
Problem, there is provided a kind of to make planting body material surface possess enough bone-inducting actives and improve bone contact ratio that built-in electric field is formed
Implantation material and preparation method thereof.
Therefore, the present invention provides a kind of implantation material for forming built-in electric field, it is by sandwich construction piezoceramic material
Composition.
Preferably, the basalis of sandwich construction is strontium titanates, and intermediate layer is ruthenic acid strontium, and top layer is bismuth ferrite.
Preferably, the implantation material that can form built-in electric field is lamellar material, and thickness is 100 μm~800 μm.
Preferably, bismuth ferrite thickness is 10 μm~80 μm.
Present invention simultaneously provides a kind of preparation method for the implantation material for forming built-in electric field, it is by pulsed laser deposition
Method is made.
Preferably, the preparation method of the implantation material provided by the invention for forming built-in electric field comprises the following steps：(1)
Substrate using strontium titanate monocrystal as electroactive implantation material, strontium titanates substrate is inserted in acetone, ethanol solution respectively successively
It is ultrasonically treated 5~10 minutes, is rinsed repeatedly with deionized water 3~5 times, is put into after nitrogen drying in 100 DEG C~150 DEG C of baking oven
Baking 3~6 hours, is cooled to room temperature；(2) the strontium titanate monocrystal substrate after the step (1) processing is taken, ruthenium is deposited on its surface
Sour strontium, its Parameter Conditions are：Laser frequency is 1~5HZ；Laser energy is 60~90mj；Partial pressure of oxygen is 10~20pa；During growth
Between be 5~30 minutes, growth temperature be 300~800 DEG C；(3) strontium titanates-ruthenic acid strontium double-decker obtained by the step (2) is taken,
Continue to deposit bismuth ferrite thin film, its Parameter Conditions on ruthenic acid strontium surface：Laser frequency is 5HZ；Laser energy is 70~90mj；Oxygen
Partial pressure is 15~20pa；Growth time is 5~60 minutes, and growth temperature is 300~800 DEG C；(4) take obtained by the step (3)
Strontium titanates-ruthenic acid strontium-bismuth ferrite three-layer structure material is dried after acetone and ethanol cleaning, obtains that built-in electric field can be formed
It is implanted into material.
The beneficial effects of the present invention are：
(1) present invention is formed with sandwich construction, including basalis strontium titanates, intermediate layer ruthenic acid strontium and top layer bismuth ferrite, shape
Into the implantation material structure stable performance for forming built-in electric field, technological parameter is controllable, has good cuttability energy,
Suitable for the bone defect healing under different condition.
(2) present invention obtained by formed built-in electric field implantation material due in bismuth ferrite polarization characteristic,
Bionical current potential that is stable, matching with natural bone tissue is produced during deposition growing.
(3) the implantation material for forming built-in electric field obtained by the present invention can promote mesenchymal stem cells MSCs in vitro
Osteoblast Differentiation, bone morphogenetic protein expression is obvious.
(4) the electroactive implantation material obtained by the present invention can be obviously promoted bone defect healing in vivo, promote early stage bone
Integrate.
(5) preparation technology tradition of the present invention is feasible, can be used for industrialized production.
In summary, the implantation material provided by the present invention for forming built-in electric field is on macro property and microstructure
Good performance is respectively provided with, in repair process is planted, the built-in electric field matched can be formed with the Cranial defect broken ends of fractured bone, stimulate new bone to give birth to
Into effective lifting early stage Integrated implant effect.
Brief description of the drawings
Fig. 1 is the built-in electric field formation basic theory signal for the implantation material that built-in electric field can be formed described in the embodiment of the present invention 1
Figure；
Fig. 2 be the embodiment of the present invention 1 described in can be formed built-in electric field implantation material polarization process ideograph (left side) and
Surface potential measurement result (right side)；
Fig. 3 is to promote BMSCs Osteoblast Differentiation bones outside the implantation material bodies for can be formed described in the embodiment of the present invention 1 built-in electric field
The immunofluorescence photograph that morphogenic protein BMP-2-2 is expressed；
Fig. 4 is that can be formed to be implanted into rat femur defect 2 inside the implantation material of built-in electric field described in the embodiment of the present invention 1
Micro-CT tri-dimensional pictures after week；
Fig. 5 is that can be formed to be implanted into rat femur defect 2 inside the implantation material of built-in electric field described in the embodiment of the present invention 1
Histological picture (hard tissue slicing, methylene blue-moral training) after week.
Embodiment
The invention provides a kind of implantation material for forming built-in electric field and preparation method thereof, below in conjunction with the accompanying drawings and has
The present invention will be further described for body embodiment.
Embodiment 1
(1) substrate using strontium titanate monocrystal as electroactive implantation material, acetone, ethanol are inserted by strontium titanates substrate successively
It is ultrasonically treated 5 minutes, is rinsed repeatedly with deionized water 3 times respectively in solution, is put into 100 DEG C of baking oven and toasts after nitrogen drying
3 hours, it is cooled to room temperature；
(2) the strontium titanate monocrystal substrate after step (1) processing is taken, ruthenic acid strontium, its Parameter Conditions are deposited on its surface：Laser
Frequency is 1HZ；Laser energy is 60mj；Partial pressure of oxygen is 10pa；Growth time is 5 minutes, and growth temperature is 300 DEG C；
(3) strontium titanates-ruthenic acid strontium double-decker obtained by taking step (2), continue to deposit bismuth ferrite thin film on ruthenic acid strontium surface,
Its Parameter Conditions：Laser frequency is 5HZ；Laser energy is 70mj；Partial pressure of oxygen is 15pa；Growth time is 5 minutes, growth temperature
For 300 DEG C；
(4) strontium titanates-ruthenic acid strontium-bismuth ferrite three-layer structure material obtained by step (3) is taken after acetone and ethanol cleaning
Dry, obtain a kind of implantation material for forming built-in electric field.
The implantation material main component for forming built-in electric field as obtained by above step is by strontium titanates, ruthenic acid strontium and iron
Sour bismuth composition, it is lamellar material, and thickness is 100 μm, and electroactive bismuth ferrite thickness degree is 10 μm.
Embodiment 2
(1) substrate using strontium titanate monocrystal as electroactive implantation material, acetone, ethanol are inserted by strontium titanates substrate successively
It is ultrasonically treated 8 minutes, is rinsed repeatedly with deionized water 4 times respectively in solution, is put into 120 DEG C of baking oven and toasts after nitrogen drying
4 hours, it is cooled to room temperature；
(2) the strontium titanate monocrystal substrate after step (1) processing is taken, ruthenic acid strontium, its Parameter Conditions are deposited on its surface：Laser
Frequency is 2HZ；Laser energy is 70mj；Partial pressure of oxygen is 15pa；Growth time is 20 minutes, and growth temperature is 500 DEG C；
(3) strontium titanates-ruthenic acid strontium double-decker obtained by taking step (2), continue to deposit bismuth ferrite thin film on ruthenic acid strontium surface,
Its Parameter Conditions：Laser frequency is 5HZ；Laser energy is 80mj；Partial pressure of oxygen is 18pa；Growth time is 30 minutes, growth temperature
Spend for 500 DEG C；
(4) strontium titanates-ruthenic acid strontium-bismuth ferrite three-layer structure material obtained by step (3) is taken after acetone and ethanol cleaning
Dry, obtain a kind of implantation material for forming built-in electric field.
The implantation material main component for forming built-in electric field as obtained by above step is by strontium titanates, ruthenic acid strontium and iron
Sour bismuth composition, it is lamellar material, and thickness is 500 μm, and electroactive bismuth ferrite thickness degree is 50 μm.
Embodiment 3
(1) substrate using strontium titanate monocrystal as electroactive implantation material, acetone, ethanol are inserted by strontium titanates substrate successively
It is ultrasonically treated respectively in solution 10 minutes, with deionized water with rinsing repeatedly, is put into 150 DEG C of baking oven and toasts after nitrogen drying
6 hours, it is cooled to room temperature；
(2) the strontium titanate monocrystal substrate after step (1) processing is taken, ruthenic acid strontium, its Parameter Conditions are deposited on its surface：Laser
Frequency is 5HZ；Laser energy is 90mj；Partial pressure of oxygen is 20pa；Growth time is 30 minutes, and growth temperature is 800 DEG C；
(3) strontium titanates-ruthenic acid strontium double-decker obtained by taking step (2), continue to deposit bismuth ferrite thin film on ruthenic acid strontium surface,
Its Parameter Conditions：Laser frequency is 5HZ；Laser energy is 90mj；Partial pressure of oxygen is 20pa；Growth time is 60 minutes, growth temperature
Spend for 800 DEG C；
The implantation material main component for forming built-in electric field as obtained by above step is by strontium titanates, ruthenic acid strontium and iron
Sour bismuth composition, it is lamellar material, and thickness is 800 μm, and electroactive bismuth ferrite thickness degree is 80 μm.
Claims (6)
- A kind of 1. implantation material for forming built-in electric field, it is characterized in that it is made up of sandwich construction piezoceramic material.
- 2. the implantation material according to claim 1 for forming built-in electric field, it is characterised in that：The base of the sandwich construction Bottom is strontium titanates, and intermediate layer is ruthenic acid strontium, and top layer is bismuth ferrite.
- 3. the implantation material according to claim 2 for forming built-in electric field, it is characterised in that：It is described to form in-built electrical The implantation material of field is lamellar material, and thickness is 100 μm~800 μm.
- 4. the implantation material according to claim 2 for forming built-in electric field, it is characterised in that：The bismuth ferrite thickness is 10 μm~80 μm.
- 5. the preparation method of the implantation material for forming built-in electric field as described in Claims 1 to 4 any one claim, It is characterized in that the implantation material for forming built-in electric field is made up of pulsed laser deposition.
- 6. the preparation method of the implantation material according to claim 5 for forming built-in electric field, it is characterised in that including such as Lower step：(1) substrate using strontium titanate monocrystal as electroactive implantation material, acetone, ethanol solution are inserted by strontium titanates substrate successively It is middle to be ultrasonically treated 5~10 minutes respectively, rinsed repeatedly with deionized water 3~5 times, 100 DEG C~150 DEG C are put into after nitrogen drying Toasted 3~6 hours in baking oven, be cooled to room temperature；(2) the strontium titanate monocrystal substrate after the step (1) processing is taken, deposits ruthenic acid strontium on its surface, its Parameter Conditions is：Swash Light frequency is 1~5HZ；Laser energy is 60~90mj；Partial pressure of oxygen is 10~20pa；Growth time is 5~30 minutes, growth temperature Spend for 300~800 DEG C；(3) strontium titanates-ruthenic acid strontium double-decker obtained by taking the step (2), continue to deposit bismuth ferrite thin film on ruthenic acid strontium surface, Its Parameter Conditions：Laser frequency is 5HZ；Laser energy is 70~90mj；Partial pressure of oxygen is 15~20pa；Growth time is 5~60 Minute, growth temperature is 300~800 DEG C；(4) strontium titanates-ruthenic acid strontium-bismuth ferrite three-layer structure material obtained by the step (3) is taken after acetone and ethanol cleaning Dry, obtain being formed the implantation material of built-in electric field.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710666015.5A CN107469150A (en) | 2017-08-07 | 2017-08-07 | A kind of implantation material for forming built-in electric field and preparation method thereof |
| PCT/CN2018/099098 WO2019029505A1 (en) | 2017-08-07 | 2018-08-07 | Implanted material capable of forming built-in electric field and preparation method therefor |
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| CN201710666015.5A CN107469150A (en) | 2017-08-07 | 2017-08-07 | A kind of implantation material for forming built-in electric field and preparation method thereof |
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| WO (1) | WO2019029505A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019029505A1 (en) * | 2017-08-07 | 2019-02-14 | 北京大学口腔医学院 | Implanted material capable of forming built-in electric field and preparation method therefor |
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| JPH02180251A (en) * | 1988-12-30 | 1990-07-13 | Kazusumi Tsutsumi | Dental implant material |
| CN1785439A (en) * | 2005-10-14 | 2006-06-14 | 哈尔滨工程大学 | Active bio piezoelectric ceramic coating layer and method of preparing said coating layer on titanium base body surface |
| US20070029592A1 (en) * | 2005-08-04 | 2007-02-08 | Ramamoorthy Ramesh | Oriented bismuth ferrite films grown on silicon and devices formed thereby |
| CN102579145A (en) * | 2012-02-23 | 2012-07-18 | 中国人民解放军第四军医大学 | Dental implant and preparation method thereof |
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| CN106047802A (en) * | 2016-06-15 | 2016-10-26 | 北京大学口腔医院 | Material for promoting mesenchymal stem cell osteoblastic differentiation and preparation method and application thereof |
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| JP5087768B2 (en) * | 2006-10-20 | 2012-12-05 | 国立大学法人 鹿児島大学 | Biocompatible high-strength ceramic composite material and manufacturing method thereof |
| CN103120805A (en) * | 2013-02-04 | 2013-05-29 | 中国科学院金属研究所 | Bioactive surface coating of biomedical degradable magnesium alloy and preparation method thereof |
| CN103272279B (en) * | 2013-04-25 | 2014-10-01 | 浙江大学 | Bioactive multilayer multiphase ceramic microsphere material and its preparation method and use |
| CN107847641A (en) * | 2015-07-28 | 2018-03-27 | 陶瓷技术有限责任公司 | Metal and/or ceramic component with least one Integrated implant and self-bone grafting surface (more) Rotating fields |
| CN107469150A (en) * | 2017-08-07 | 2017-12-15 | 北京大学口腔医学院 | A kind of implantation material for forming built-in electric field and preparation method thereof |
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2017
- 2017-08-07 CN CN201710666015.5A patent/CN107469150A/en active Pending
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2018
- 2018-08-07 WO PCT/CN2018/099098 patent/WO2019029505A1/en active Application Filing
Patent Citations (7)
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|---|---|---|---|---|
| JPH02180251A (en) * | 1988-12-30 | 1990-07-13 | Kazusumi Tsutsumi | Dental implant material |
| US20070029592A1 (en) * | 2005-08-04 | 2007-02-08 | Ramamoorthy Ramesh | Oriented bismuth ferrite films grown on silicon and devices formed thereby |
| CN1785439A (en) * | 2005-10-14 | 2006-06-14 | 哈尔滨工程大学 | Active bio piezoelectric ceramic coating layer and method of preparing said coating layer on titanium base body surface |
| CN102579145A (en) * | 2012-02-23 | 2012-07-18 | 中国人民解放军第四军医大学 | Dental implant and preparation method thereof |
| CN102586747A (en) * | 2012-03-13 | 2012-07-18 | 浙江理工大学 | Preparation method of (BiFe03) m/(La0.7Sr0.3Mn03)n multi-layer film |
| CN104726836A (en) * | 2013-12-20 | 2015-06-24 | 中国科学院上海硅酸盐研究所 | Titanium metal material surface modifying method and modified titanium metal material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019029505A1 (en) * | 2017-08-07 | 2019-02-14 | 北京大学口腔医学院 | Implanted material capable of forming built-in electric field and preparation method therefor |
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Application publication date: 20171215 |